تفاعل #3659

معادلة التفاعل

10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine

4-[N-methyl-N-(2-methylbenzoyl)amino]benzoyl chloride

triethylamine

tetrahydrofuran

4-[N-methyl-N-(2-methylbenzoyl)amino]benzoyl chloride

triethylamine

→

crystals

المردود 59.5%

N-[4-(5H-Pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]-N-methyl-2-methylbenzamide

المردود 59.5%

المذيبات

water

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGthe mixture stirred for 2 days
2. 2
   استخلاصextracted with dichloromethane
3. 3
   غسيلThe extract is washed with water, 1N HCl, 1N NaHCO3, brine
4. 4
   تجفيفdried (Na2SO4)
5. 5
   ترشيحThe solution is filtered through a thin pad of hydrous magnesium silicate
6. 6
   أخرىThe filtrate is evaporated in vacuo
7. 7
   أخرىthe residue crystallized from dichloromethane-hexane

الإجراء التجريبي

A mixture of 0.27 g of 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 0,518 g of 4-[N-methyl-N-(2-methylbenzoyl)amino]benzoyl chloride, 0.182 g of triethylamine and 7 ml of tetrahydrofuran is stirred at room temperature for 3 hours. To the mixture is added 0.29 g of 4-[N-methyl-N-(2-methylbenzoyl)amino]benzoyl chloride and 0.10 g of triethylamine in 2 ml of dichloromethane and the mixture stirred for 2 days. The mixture is poured into water and extracted with dichloromethane. The extract is washed with water, 1N HCl, 1N NaHCO3, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrous magnesium silicate. The filtrate is evaporated in vacuo and the residue crystallized from dichloromethane-hexane to give 0.38 g of crystals, m.p. 168°-170° C.

المصدر